CN109273377A - Preprocess method before the detection at monocrystalline silicon concentric circles and black angle - Google Patents

Preprocess method before the detection at monocrystalline silicon concentric circles and black angle Download PDF

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Publication number
CN109273377A
CN109273377A CN201811020607.0A CN201811020607A CN109273377A CN 109273377 A CN109273377 A CN 109273377A CN 201811020607 A CN201811020607 A CN 201811020607A CN 109273377 A CN109273377 A CN 109273377A
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Prior art keywords
print
monocrystalline silicon
acid solution
detection
sample block
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CN201811020607.0A
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CN109273377B (en
Inventor
张浩强
杨红涛
柳志强
杨建勇
焦鹏
李双凯
李春辉
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Qujing Jingao Photovoltaic Technology Co ltd
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NINGJIN JINGXING ELECTRONIC MATERIAL CO Ltd
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    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01LSEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L22/00Testing or measuring during manufacture or treatment; Reliability measurements, i.e. testing of parts without further processing to modify the parts as such; Structural arrangements therefor
    • H01L22/10Measuring as part of the manufacturing process
    • H01L22/12Measuring as part of the manufacturing process for structural parameters, e.g. thickness, line width, refractive index, temperature, warp, bond strength, defects, optical inspection, electrical measurement of structural dimensions, metallurgic measurement of diffusions
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01LSEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L22/00Testing or measuring during manufacture or treatment; Reliability measurements, i.e. testing of parts without further processing to modify the parts as such; Structural arrangements therefor
    • H01L22/10Measuring as part of the manufacturing process
    • H01L22/14Measuring as part of the manufacturing process for electrical parameters, e.g. resistance, deep-levels, CV, diffusions by electrical means
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01LSEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L22/00Testing or measuring during manufacture or treatment; Reliability measurements, i.e. testing of parts without further processing to modify the parts as such; Structural arrangements therefor
    • H01L22/20Sequence of activities consisting of a plurality of measurements, corrections, marking or sorting steps

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  • Engineering & Computer Science (AREA)
  • Manufacturing & Machinery (AREA)
  • Computer Hardware Design (AREA)
  • Microelectronics & Electronic Packaging (AREA)
  • Power Engineering (AREA)
  • Testing Or Measuring Of Semiconductors Or The Like (AREA)

Abstract

The present invention relates to preprocess methods before a kind of detection of monocrystalline silicon concentric circles, cut the sample block of monocrystalline silicon head circular;The monocrystalline silicon head sample block that will acquire cuts out the print of 1/4 circle or more with diamond pen;The print annealing that will acquire;Print after annealing is cooked by alkaline solution;Then the print after cooking is dipped into acid solution;By impregnate acid solution after print pure water rinsing, dry;The print dried is subjected to print minority carrier lifetime.The present invention also provides preprocess methods before a kind of detection at the black angle of monocrystalline silicon, cut any monocrystalline silicon tail portion circle sample block;The monocrystalline silicon head sample block that will acquire cuts out the print of 1/3 circle or more with diamond pen;The print acid solution corrosion that will acquire;Print cleaning acid solution residual after acid solution is corroded;The remaining print annealing of acid solution will be cleaned;After the print natural air drying of annealing, cooked using alkaline solution;Treated print will be cooked and carry out minority carrier lifetime.

Description

Preprocess method before the detection at monocrystalline silicon concentric circles and black angle
Technical field
The present invention relates to vertical pulling method field of single crystal growth and field of semiconductor manufacture, more particularly to monocrystalline silicon is same Preprocess method before the detection at heart circle and black angle.
Background technique
With the rapid development of monocrystalline silicon photovoltaic industry, monocrystalline silicon yield increases year by year;And monocrystalline silicon photovoltaic is turned Efficiency is changed increasingly to improve, it is higher and higher to monocrystalline silicon quality requirements.
And the concentric circles of monocrystalline silicon, Hei Jiao (black surround) defect seriously affect the transfer efficiency of photovoltaic;Wherein concentric circles are as follows: single Crystal silicon chip is tested by EL tester, and due to existing defects inside silicon wafer, when test is in circular ring shape at silicon wafer center, referred to as together Heart circle.Concentric circles producing cause is: during crystal for straight drawing monocrystal growth, between gap enrichment region and vacancy enrichment region It will form annular section, if oxygen content is increased to certain level, will form vacancy oxygen defect ring;Vacancy oxygen defect ring position exists It will form Thermal donor in crystal cooling procedure, influence minority carrier life time;And crystal bar head oxygen content is higher, general vacancy oxygen defect ring It is obvious in crystal bar head position.Black angle are as follows: monocrystalline silicon piece is tested by EL tester, due to silicon wafer internal flaw, tests four Corner blacks, referred to as black angle.Black angle producing cause: being produced from interstitial silicon atoms in the aerobic heat treatment process of monocrystalline, from surface to Oxidation stacking fault is diffuseed to form in vivo, performance becomes apparent from crystal bar tail portion.Wherein EL tester be a kind of solar battery or electricity The Inner Defect Testing equipment of pond component.
The concentric circles of monocrystalline silicon and black angular defect are easy to cause monocrystalline silicon quality to be deteriorated, and color difference is formed in single crystal silicon product The problems such as, the performance of crystalline silicon and device has been seriously affected, the photoelectric conversion efficiency of silicon solar cell is reduced;Currently without A kind of effective detection mode, judge monocrystalline silicon exemplar concentric circles and black angular defect.
Therefore, how to provide a kind of method for being capable of detecting when monocrystalline silicon concentric circles and black angular defect is those skilled in the art The problem of member's urgent need to resolve.
Summary of the invention
In view of this, being capable of detecting when the present invention provides a kind of monocrystalline silicon concentric circles and the detection method of black angular defect Concentric circles and black angular defect, improve the ex factory pass rate of monocrystalline silicon.
To achieve the goals above, the present invention adopts the following technical scheme:
Preprocess method before the detection of monocrystalline silicon concentric circles provided by the invention, comprising the following steps:
S1, the sample block for cutting monocrystalline silicon head circular;
S2, the print that the monocrystalline silicon head sample block obtained in S1 is cut out to 1/4 circle or more with diamond pen;
S3, the print obtained in S2 is made annealing treatment;
S4, the print after making annealing treatment in S3 is cooked by alkaline solution;
S5, then by S4 cook after print be dipped into acid solution;
S6, by S5 impregnate acid solution after print through pure water rinsing, dry;
S7, the print dried in S6 is subjected to print minority carrier lifetime.
It can be seen via above technical scheme that compared with prior art, the present disclosure provides a kind of monocrystalline silicon is concentric Preprocess method before round detection, is made annealing treatment before testing, is conducive to the diffusion of impurity in monocrystalline silicon (oxygen), then It is handled by alkaline solution cooking, sloughs the oxidation film of sample surface.It is remained in acid soak with alkali, is examining the defect of print Surveying under instrument can show, and improve the precision of the internal flaw of the print of measurement, and then effectively control product export qualification Rate.
Sample surface life test can be carried out using Hungary WT2000PVN minority carrier lifetime tester.
Preferably, the sample block diameter that monocrystalline silicon head circular is cut in S1 is 210-216mm, with a thickness of 0.8-1.5mm; Facilitate cutting and meets test needs.
Preferably, it is 600-1000 DEG C that temperature is made annealing treatment in S3, and constant temperature 1-2.5h.Wherein monocrystalline silicon is at different warm Phenomena such as under the conditions of reason, extremely complex thermal behavior is presented in oxygen in silicon, will form Thermal donor, oxygen precipitation.Oxygen precipitation is usually Electrically inactive, but it can be formed together network and object with some metal impurities, the present invention passes through the height to print with induced defects Warm processing amplifies the defect on print, it is easier to monocrystalline silicon internal flaw is detected under detecting instrument.
Preferably, S4 neutral and alkali solution quality percent concentration is the sodium hydroxide solution of 20-25%, brew temperatures 80- 100 DEG C, brew time 10-40min.
Preferably, acid solution concentration of volume percent is the hydrofluoric acid of 2-3%, soaking time 10-12min.
The present invention provides preprocess methods before the detection at the black angle of monocrystalline silicon, comprising the following steps:
A1, monocrystalline silicon tail portion circle sample block is cut;
A2, the print that the monocrystalline silicon head sample block obtained in A1 is cut out to 1/3 circle or more with diamond pen;
A3, the print acid solution obtained in A2 is corroded;
A4, the print cleaning acid solution after acid solution corrosion in A3 is remained;
A5, the remaining print annealing of acid solution will be cleaned in A4;
A6, by after the print natural air drying made annealing treatment in A5, cooked using alkaline solution;
A7, treated print will be cooked in A6 and carry out minority carrier lifetime;
Wherein A3-A5 needs operating personnel with good protection tool, and sample is slowly put into acid solution one by one and is corroded;To corruption After erosion, print is taken out from acid corrosion environment immediately, is cleaned in the sink with the pure water of flowing, is put into quartz boat after drying In must not squeeze, then anneal after furnace temperature reaches, quartz boat be put into annealing furnace and is annealed.
It after print air-dries after annealing in A6, is sequentially placed into basketry, then basketry is put into alkaline solution and is cooked, be passivated Processing, is dried at ultrasonic cleaning, is then placed in the polybag of Self-enclosing, and internal drum is discharged, and is sent to life test rack progress Detection.
Hungary WT2000PVN minority carrier lifetime tester test sample surface lifetime can be used in A7.It is (above-mentioned single Step is identical as monocrystalline silicon concentric circles test, is only that test monocrystalline silicon concentric circles is different from the specific sequence of steps in black angle.)
It can be seen via above technical scheme that compared with prior art, the present disclosure provides a kind of black angles of monocrystalline silicon Detection method, the present invention first pass through to print acid solution burn into removes surface impurity, grinding damage layer and formed corrosion Hole, then removes acidic residual, is being made annealing treatment, make the impurity diffusion in exemplar, is deviate from after air-drying by alkaline solution Then oxidation film carries out exemplar minority carrier lifetime.
Preferably, it is 210-216mm that the circular sample block diameter in monocrystalline silicon tail portion is cut in A1, with a thickness of 0.8-1.5mm; Facilitate cutting and meets test needs.
Preferably, acid solution is hydrofluoric acid, nitric acid and water according to the acid solution that weight ratio is that 1:3:9 is configured in A3.
Preferably, in A5 in annealing, annealing temperature is 700-950 DEG C, constant temperature time 1-3h.
Preferably, A6 neutral and alkali solution quality percent concentration is 20-25% sodium hydroxide solution, brew temperatures 80- 100 DEG C, brew time 10-40min.
Detailed description of the invention
In order to more clearly explain the embodiment of the invention or the technical proposal in the existing technology, to embodiment or will show below There is attached drawing needed in technical description to be briefly described, it should be apparent that, the accompanying drawings in the following description is only this The embodiment of invention for those of ordinary skill in the art without creative efforts, can also basis The attached drawing of offer obtains other attached drawings.
Fig. 1 attached drawing is the concentric circles electron microscope that method provided by the invention detects;
Fig. 2 attached drawing is non-concentric electron microscope;
Fig. 3 attached drawing is the electron microscope at the black angle that method provided by the invention detects;
Fig. 4 attached drawing is the electron microscope at non-black angle;
Fig. 5, Fig. 6 attached drawing are the test electron microscope without the print of processing.
Specific embodiment
Following will be combined with the drawings in the embodiments of the present invention, and technical solution in the embodiment of the present invention carries out clear, complete Site preparation description, it is clear that described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.It is based on Embodiment in the present invention, it is obtained by those of ordinary skill in the art without making creative efforts every other Embodiment shall fall within the protection scope of the present invention.
The embodiment of the invention discloses a kind of monocrystalline silicon concentric circles and the detection method of black angular defect, it is capable of detecting when with one heart Round and black angular defect, improves the ex factory pass rate of monocrystalline silicon.
Embodiment 1
Preprocess method before the detection of monocrystalline silicon concentric circles provided by the invention, comprising the following steps:
S1, sample block the diameter 210mm, thickness 0.8mm for cutting monocrystalline silicon head circular;
S2, the print that the monocrystalline silicon head sample block obtained in S1 is cut out to 1/4 circle or more with diamond pen;
S3, the print obtained in S2 is made annealing treatment, annealing temperature is 600 DEG C, constant temperature 1h;
S4, the print after making annealing treatment in S3 is cooked by the sodium hydroxide solution that mass percent concentration is 20%, 80 DEG C of brew temperatures, brew time 10min;
S5, then by S4 cook after print be dipped into concentration of volume percent be 2% hydrofluoric acid solution in 10min;
S6, by S5 impregnate acid solution after print through pure water rinsing, dry;
S7, the print after drying in S6 is subjected to the sample surface longevity using Hungary WT2000PVN minority carrier lifetime tester Life test.
Embodiment 2
Preprocess method before the detection of monocrystalline silicon concentric circles provided by the invention, comprising the following steps:
S1, sample block the diameter 214mm, thickness 1.2mm for cutting monocrystalline silicon head circular;
S2, the print that the monocrystalline silicon head sample block obtained in S1 is cut out to 1/4 circle or more with diamond pen;
S3, the print obtained in S2 is made annealing treatment, annealing temperature is 800 DEG C, constant temperature 2h;
S4, the print after making annealing treatment in S3 is cooked by the sodium hydroxide solution that mass percent concentration is 23%, 90 DEG C of brew temperatures, brew time 25min;
S5, then by S4 cook after print be dipped into concentration of volume percent be 2% hydrofluoric acid solution in 11min;
S6, by S5 impregnate acid solution after print through pure water rinsing, dry;
S7, the print after drying in S6 is subjected to the sample surface longevity using Hungary WT2000PVN minority carrier lifetime tester Life test.
Embodiment 3
Preprocess method before the detection of monocrystalline silicon concentric circles provided by the invention, comprising the following steps:
S1, sample block the diameter 216mm, thickness 1.5mm for cutting monocrystalline silicon head circular;
S2, the print that the monocrystalline silicon head sample block obtained in S1 is cut out to 1/4 circle or more with diamond pen;
S3, the print obtained in S2 is made annealing treatment, annealing temperature is 1000 DEG C, constant temperature 2.5h;
S4, the print after making annealing treatment in S3 is cooked by the sodium hydroxide solution that mass percent concentration is 25%, 100 DEG C of brew temperatures, brew time 40min;
S5, then by S4 cook after print be dipped into concentration of volume percent be 3% hydrofluoric acid solution in 12min;
S6, by S5 impregnate acid solution after print through pure water rinsing, dry;
S7, the print after drying in S6 is subjected to the sample surface longevity using Hungary WT2000PVN minority carrier lifetime tester Life test.
Embodiment 4
The present invention provides preprocess methods before the detection at the black angle of monocrystalline silicon, comprising the following steps:
A1, monocrystalline silicon tail portion circle sample block diameter 210mm, thickness 0.8mm are cut;
A2, the print that the monocrystalline silicon head sample block obtained in A1 is cut out to 1/3 circle or more with diamond pen;
A3, the print acid solution obtained in A2 is corroded, it according to weight ratio is 1:3 that acid solution, which is hydrofluoric acid, nitric acid and water: The solution of 9 configurations;
A4, the print cleaning acid solution after acid solution corrosion in A3 is remained;
A5, it the remaining print of cleaning acid solution will be made annealing treatment in A4,700 DEG C of annealing temperature, constant temperature 1h;
A6, by after the print natural air drying made annealing treatment in A5, the use of mass percent concentration is that 20% sodium hydroxide is molten Liquid alkaline solution cooks, and 80 DEG C of brew temperatures, brew time 10min;
A7, treated print will be cooked in A6 and carry out minority carrier lifetime.
Embodiment 5
The present invention provides preprocess methods before the detection at the black angle of monocrystalline silicon, comprising the following steps:
A1, monocrystalline silicon tail portion circle sample block diameter 214mm, thickness 1.2mm are cut;
A2, the print that the monocrystalline silicon head sample block obtained in A1 is cut out to 1/3 circle or more with diamond pen;
A3, the print acid solution obtained in A2 is corroded, it according to weight ratio is 1:3 that acid solution, which is hydrofluoric acid, nitric acid and water: The solution of 9 configurations;
A4, the print cleaning acid solution after acid solution corrosion in A3 is remained;
A5, it the remaining print of cleaning acid solution will be made annealing treatment in A4,850 DEG C of annealing temperature, constant temperature 2h;
A6, by after the print natural air drying made annealing treatment in A5, the use of mass percent concentration is that 23% sodium hydroxide is molten Liquid alkaline solution cooks, and 90 DEG C of brew temperatures, brew time 35min;
A7, treated print will be cooked in A6 and carry out minority carrier lifetime.
Embodiment 6
The present invention provides preprocess methods before the detection at the black angle of monocrystalline silicon, comprising the following steps:
A1, monocrystalline silicon tail portion circle sample block diameter 216mm, thickness 1.5mm are cut;
A2, the print that the monocrystalline silicon head sample block obtained in A1 is cut out to 1/3 circle or more with diamond pen;
A3, the print acid solution obtained in A2 is corroded, it according to weight ratio is 1:3 that acid solution, which is hydrofluoric acid, nitric acid and water: The solution of 9 configurations;
A4, the print cleaning acid solution after acid solution corrosion in A3 is remained;
A5, it the remaining print of cleaning acid solution will be made annealing treatment in A4,950 DEG C of annealing temperature, constant temperature 3h;
A6, by after the print natural air drying made annealing treatment in A5, the use of mass percent concentration is that 25% sodium hydroxide is molten Liquid alkaline solution cooks, and 100 DEG C of brew temperatures, brew time 40min;
A7, treated print will be cooked in A6 and carry out minority carrier lifetime.
Comparative example 1
Using the print after cutting without any processing, directly measurement monocrystalline silicon print concentric circles and black angular defect.
Comparative example 2
Print is handled using the method that approximate processing monocrystalline silicon print measures black angle, measures concentric circles;The following steps are included:
Cut sample block the diameter 216mm, thickness 1.5mm of monocrystalline silicon head circular;
The monocrystalline silicon head sample block that will acquire cuts out the print of 1/4 circle or more with diamond pen;
The print acid solution corrosion that will acquire, it is 1:3:9 configuration that acid solution, which is hydrofluoric acid, nitric acid and water according to weight ratio, Solution;
Print cleaning acid solution residual after acid solution is corroded;
The remaining print of acid solution will be cleaned to make annealing treatment, 700 DEG C of annealing temperature, constant temperature 1h;
It the use of mass percent concentration is that 20% sodium hydroxide solution alkalinity is molten after the print natural air drying of annealing Liquid cooks, and 80 DEG C of brew temperatures, brew time 10min;
Treated print will be cooked and carry out minority carrier lifetime.
Comparative example 3
Print is handled using the method for approximate processing monocrystalline silicon print measurement concentric circles, measures the black angular defect of monocrystalline silicon;Packet Include following steps:
Cut monocrystalline silicon tail portion circle sample block diameter 210mm, thickness 0.8mm;
The monocrystalline silicon head sample block that will acquire cuts out the print of 1/3 circle or more with diamond pen;
The print obtained in S2 is made annealing treatment, annealing temperature is 600 DEG C, constant temperature 1h;
Print after annealing is cooked by the sodium hydroxide solution that mass percent concentration is 20%, brew temperatures 80 DEG C, brew time 10min;
Then the print after cooking is dipped into 10min in the hydrofluoric acid solution that concentration of volume percent is 2%;
By impregnate acid solution after print through pure water rinsing, dry;
Print after drying is subjected to sample surface life test using Hungary WT2000PVN minority carrier lifetime tester.
Experimental study:
Print, each implementation are handled according to the step of embodiment 1-3, comparative example 2 using identical equipment and solution ratio The corresponding one group of print of example, every group of radix are that 100 prints carry out the processing of corresponding embodiment mode;Comparative example 1 does not do any place Reason is cut into 100 above prints of 1/4 circle;Then by the corresponding print in 5 embodiments, every group is picked out 20 at random A print carries out minority carrier lifetime, testing procedure by Hungary WT2000PVN are as follows: booting connection wiring harness, preheating;Setting-out Piece, carry out the scanning of print service life, be scanned with 1 stride, sweep parameter be respectively provided with it is identical do not change, tested;Test Afterwards by print take out save, then compared with standard data by data, judge whether this print has concentric circles, and so on survey Examination.Result after test is referring to table one:
The random model machine Detection accuracy table of table one, concentric circles
Whether can understand and tell concentric circles Detect concentric circles accuracy rate
Embodiment 1 It is 93.1%
Embodiment 2 It is 95.7%
Embodiment 3 It is 94.2%
Comparative example 1 It is no 0.0%
Comparative example 2 It can not clearly show that 20.3%
It can clearly be distinguished by the processing method that table one and attached drawing 1-2 can be seen that 1-3 through the embodiment of the present invention Whether Chu not have concentric circles, test sample, can be effective for whether there is Concentric circles detection accuracy rate to be above 90% Prevent rejected product from dispatching from the factory;And comparative example 1 can not be shown without the print of any step process in tester referring to attached drawing 5 Defect;The print that comparative example 2 is handled in the way of detecting black angle, can not clearly show that, accuracy rate is low, can not effectively rise It is acted on to quality inspection.
Print, each implementation are handled according to the step of embodiment 4-6, comparative example 3 using identical equipment and solution ratio The corresponding one group of print of example, every group of radix are that 100 prints carry out the processing of corresponding embodiment mode;Comparative example 1 does not do any place Reason is cut into 100 above prints of 1/3 circle;Then by the corresponding print in 5 embodiments, every group is picked out 20 at random A print carries out minority carrier lifetime, testing procedure by Hungary WT2000PVN are as follows: booting connection wiring harness, preheating;Setting-out Piece, carry out the scanning of print service life, be scanned with 1 stride, sweep parameter be respectively provided with it is identical do not change, tested;Test Afterwards by print take out save, then compared with standard data by data, judge whether this print has black angle, and so on survey Examination.Result after test is referring to table two:
Table two, the random model machine Detection accuracy table in black angle
Whether can understand and tell black angle Detect black angle accuracy rate
Embodiment 4 It is 92.5%
Embodiment 5 It is 97.0%
Embodiment 6 It is 96.5%
Comparative example 1 It is no 0.0%
Comparative example 3 It can not clearly show that 40.1%
By table two and attached drawing 3-4 it can be seen that the processing method of 4-6 can clearly divide through the embodiment of the present invention Whether have black angle, whether test sample can effectively prevent for there is black angle Detection accuracy to be above 90% if discerning Rejected product factory;Referring to attached drawing 6, and comparative example 1 without any step process print tester can not display defect; The print that comparative example 3 is handled in the way of detecting concentric circles can not clearly show that, accuracy rate is low, can not effectively play Quality inspection effect.
Each embodiment in this specification is described in a progressive manner, the highlights of each of the examples are with other The difference of embodiment, the same or similar parts in each embodiment may refer to each other.For device disclosed in embodiment For, since it is corresponded to the methods disclosed in the examples, so being described relatively simple, related place is said referring to method part It is bright.
The foregoing description of the disclosed embodiments enables those skilled in the art to implement or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, as defined herein General Principle can be realized in other embodiments without departing from the spirit or scope of the present invention.Therefore, of the invention It is not intended to be limited to the embodiments shown herein, and is to fit to and the principles and novel features disclosed herein phase one The widest scope of cause.

Claims (10)

1. preprocess method before the detection of monocrystalline silicon concentric circles, which comprises the following steps:
S1, the sample block for cutting any monocrystalline silicon head circular;
S2, the print that the monocrystalline silicon head sample block obtained in S1 is cut out to 1/4 circle or more with diamond pen;
S3, the print obtained in S2 is made annealing treatment;
S4, the print after making annealing treatment in S3 is cooked by alkaline solution;
S5, then by S4 cook after print be dipped into acid solution;
S6, by S5 impregnate acid solution after print through pure water rinsing, dry;
S7, the print dried in S6 is subjected to print minority carrier lifetime.
2. preprocess method before the detection of monocrystalline silicon concentric circles according to claim 1, which is characterized in that cut list in S1 The sample block diameter of crystal silicon head circular is 210-216mm, with a thickness of 0.8-1.5mm.
3. preprocess method before the detection of monocrystalline silicon concentric circles according to claim 1, which is characterized in that in S3 at annealing Managing temperature is 600-1000 DEG C, and constant temperature 1-2.5h.
4. preprocess method before the detection of monocrystalline silicon concentric circles according to claim 1, which is characterized in that S4 neutral and alkali is molten Liquid mass percent concentration be 20-25% sodium hydroxide solution, 80-100 DEG C of brew temperatures, brew time 10-40min.
5. preprocess method before the detection of monocrystalline silicon concentric circles according to claim 1, which is characterized in that acid solution volume Percent concentration is the hydrofluoric acid of 2-3%, soaking time 10-12min.
6. preprocess method before the detection at the black angle of monocrystalline silicon, which comprises the following steps:
A1, any monocrystalline silicon tail portion circle sample block is cut;
A2, the print that the monocrystalline silicon head sample block obtained in A1 is cut out to 1/3 circle or more with diamond pen;
A3, the print acid solution obtained in A2 is corroded;
A4, the print cleaning acid solution after acid solution corrosion in A3 is remained;
A5, the remaining print annealing of acid solution will be cleaned in A4;
A6, by after the print natural air drying made annealing treatment in A5, cooked using alkaline solution;
A7, treated print will be cooked in A6 and carry out minority carrier lifetime.
7. preprocess method before the detection at the black angle of monocrystalline silicon according to claim 6, which is characterized in that cut monocrystalline in A1 The circular sample block diameter in silicon tail portion is 210-216mm, with a thickness of 0.8-1.5mm.
8. preprocess method before the detection at the black angle of monocrystalline silicon according to claim 6, which is characterized in that acid solution in A3 For hydrofluoric acid, nitric acid and water according to weight ratio be 1:3:9 configuration acid solution.
9. preprocess method before the detection at the black angle of monocrystalline silicon according to claim 6, which is characterized in that made annealing treatment in A5 In, annealing temperature is 700-950 DEG C, constant temperature time 1-3h.
10. preprocess method before the detection at the black angle of monocrystalline silicon according to claim 6, which is characterized in that A6 neutral and alkali is molten Liquid mass percent concentration be 20-25% sodium hydroxide solution, 80-100 DEG C of brew temperatures, brew time 10-40min.
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Cited By (3)

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CN109860040A (en) * 2019-01-30 2019-06-07 西安奕斯伟硅片技术有限公司 Silicon etch process, silico briquette, pulling of crystals method of pulling up and monocrystalline
CN110561200A (en) * 2019-08-02 2019-12-13 菲特晶(南京)电子有限公司 quartz wafer processing technology
CN115832101A (en) * 2022-11-04 2023-03-21 隆基绿能科技股份有限公司 Pretreatment method of solar cell and silicon wafer abnormity detection method

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